制备高氯酸铵

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%7B%22isDisplay%22%3Atrue%7D

Vanguard_Marx 浪迹天涯

1年6个月前 IP:福建

D861876

1楼

使用此方法得到的产物纯度是多少 sticker

零产率人

作者

1年6个月前 IP:河北

D861924

2楼

引用Vanguard_Marx发表于1楼的内容

使用此方法得到的产物纯度是多少

工业级，纯度很渣渣

D861930

3楼

指第一种方法

MARK_GYC

1年5个月前 IP:北京

D863290

4楼

问题是NaClO4是怎么来的？我猜lz肯定有证吧

1年5个月前 IP:河北

D863298

5楼

引用MARK_GYC发表于4楼的内容

问题是NaClO4是怎么来的？我猜lz肯定有证吧

自己电解

D863309

6楼

引用零产率人发表于5楼的内容

自己电解

（棒！）这纯度肯定混不错的吧

D863317

8楼

如果按照5v20安培的电流进行电解一升的氯酸钠饱和溶液，阳极使用惰性电极，这至少要多少天才能将正五价氯离子全部氧化为正七价氯离子

D863384

9楼

引用MARK_GYC发表于8楼的内容

如果按照5v20安培的电流进行电解一升的氯酸钠饱和溶液，阳极使用惰性电极，这至少要多少天才能将正五价氯离子全部氧化为正七价氯离子

一般直接电解，连续电解两天之后高氯酸钠析出

D863410

10楼

引用零产率人发表于9楼的内容

一般直接电解，连续电解两天之后高氯酸钠析出

你好，我也刚买了些NaClO3，准备电解制NaClO4和NH4ClO4.但您也说过不纯净（混有氯酸钠）的NaClO4与NH4Cl复分解会产生更易爆的NH4ClO3,威胁到我们实验者的人生安全,

所以为了尽可能得更高纯度的NH4ClO4,按照这种速率，至少要多少天时间才能尽量去除残留的NaClO3？或是如何检验ClO3-离子，谢谢！

D863429

11楼

检测的话需要色谱分析法

D863432

13楼

电解的话析出结晶之后再重结晶一下也可以，而且直接制备出来的高氯酸铵不能直接用如果用的话害得用丙酮溶解，然后搅拌下加入乙酸乙酯析出高氯酸铵结晶

D863448

引用MARK_GYC发表于10楼的内容

你好，我也刚买了些NaClO3，准备电解制NaClO4和NH4ClO4.但您也说过不纯净（混有氯酸钠）的NaClO4与NH4Cl复分解会产生更易爆的NH4ClO3,威胁到我们实验者的人生安全, ...

我发现氯酸钠和高氯酸钠可以用乙醇分离，把高氯酸钠过量溶于乙醇后将不溶物扔掉，然后蒸馏掉乙醇

D863451

14楼

引用零产率人发表于13楼的内容

我发现氯酸钠和高氯酸钠可以用乙醇分离，把高氯酸钠过量溶于乙醇后将不溶物扔掉，然后蒸馏掉乙醇

用这种方法，是不是乙醇的浓度越高越好？这样就可以尽可能的提纯高氯酸钠（90%的纯度以上），然后直接制备高氯酸铵？

D863452

15楼

引用零产率人发表于13楼的内容

电解的话析出结晶之后再重结晶一下也可以，而且直接制备出来的高氯酸铵不能直接用如果用的话害得用丙酮溶解，然后搅拌下加入乙酸乙酯析出高氯酸铵结晶

为什么还要这一步？况且丙酮现在还因为管制而难以购买，您可以详细说明不能直接使用电解出来的高氯酸铵的原因？谢谢

D863468

16楼

引用MARK_GYC发表于15楼的内容

为什么还要这一步？况且丙酮现在还因为管制而难以购买，您可以详细说明不能直接使用电解出来的高氯酸铵的原因？谢谢

一般不是球ap他不稳定，球ap相对于直接制备出来的ap稳定一些，丙酮的话可以用硫酸溶解三氧化铬然后氧化异丙醇，蒸馏出来产物就是丙酮，副产物是硫酸铬

D863469

17楼

最好直接买无水乙醇

D863470

18楼

而且这么做可以提高ap的纯度

D863839

19楼

引用零产率人发表于2楼的内容

工业级，纯度很渣渣

我看0℃时高氯酸铵的溶解度比氯化钠溶解度更低，经过计算在0摄氏度（假设因为盐的存在导致此是水呈液态）时过滤（或抽滤）回收高氯酸铵的纯度可以达到83%，所以可以尝试在零度抽滤吗？（过滤仪器经过预冷）

最棘手的问题就是我不知道有什么好办法可以分离高氯酸铵和氯化钠（有没有一种溶剂可以溶解大量氯化钠或者高氯酸铵，然后再蒸馏）

如果都不行，可以试试直接用硫酸来蒸馏出高氯酸再与其他铵盐反应吗？期待楼主回复！谢谢！

D863855

20楼

引用MARK_GYC发表于19楼的内容

我看0℃时高氯酸铵的溶解度比氯化钠溶解度更低，经过计算在0摄氏度（假设因为盐的存在导致此是水呈液态）时过滤（或抽滤）回收高氯酸铵的纯度可以达到83%，所以可以尝试在零度抽滤吗？（过滤仪器经过预冷）最棘...

抽滤的话肯定是可以的，另外氯化钠不溶于大部分的有机溶剂，可以试试把粗制高氯酸铵过量丙酮溶解，然后抽滤，在溶解了高氯酸铵的丙酮中剧烈搅拌中加入乙酸乙酯，这种方法得到的高氯酸铵做火箭燃料即可，然后溶剂蒸馏回收就行了

D863863

21楼

引用零产率人发表于20楼的内容

抽滤的话肯定是可以的，另外氯化钠不溶于大部分的有机溶剂，可以试试把粗制高氯酸铵过量丙酮溶解，然后抽滤，在溶解了高氯酸铵的丙酮中剧烈搅拌中加入乙酸乙酯，这种方法得到的高氯酸铵做火箭燃料即可，然后溶剂蒸馏...

OK，我先用无水乙醇分离高氯酸钠，然后再用降温过滤进一步提纯高氯酸铵，最后用丙酮分离氯化钠，这样纯度应该完美吧

D863872

25楼

引用零产率人发表于24楼的内容

可以，高氯酸铵溶解后最好用乙酸乙酯让高氯酸铵析出，然后干燥的话我选用减压蒸馏，有钱用旋蒸也可以。

为什么要用乙酸乙酯？这样做不就增加分离丙酮和乙酸乙酯的复杂度吗？并且我想补充一下粉碎AP的过程如何确保安全（防止自燃）？您可以详细的告诉我使用乙酸乙酯分离高氯酸铵的原理吗（还有最后如何分离丙酮和乙酸乙酯），我还是有点不太懂您的方式，毕竟我才刚准备入门……

D863877

24楼

引用MARK_GYC发表于21楼的内容

OK，我先用无水乙醇分离高氯酸钠，然后再用降温过滤进一步提纯高氯酸铵，最后用丙酮分离氯化钠，这样纯度应该完美吧

可以，高氯酸铵溶解后最好用乙酸乙酯让高氯酸铵析出，然后干燥的话我选用减压蒸馏，有钱用旋蒸也可以。

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26楼

引用MARK_GYC发表于25楼的内容

为什么要用乙酸乙酯？这样做不就增加分离丙酮和乙酸乙酯的复杂度吗？并且我想补充一下粉碎AP的过程如何确保安全（防止自燃）？您可以详细的告诉我使用乙酸乙酯分离高氯酸铵的原理吗（还有最后如何分离丙酮和乙酸乙...

高氯酸铵溶于丙酮不溶于乙酸乙酯，这样可以析出高氯酸铵，而且制作出来的高氯酸铵不用粉碎细度高，回收丙酮和乙酸乙酯蒸馏就行用沸点的不同分离出来

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引用零产率人发表于26楼的内容

高氯酸铵溶于丙酮不溶于乙酸乙酯，这样可以析出高氯酸铵，而且制作出来的高氯酸铵不用粉碎细度高，回收丙酮和乙酸乙酯蒸馏就行用沸点的不同分离出来

谢谢您一直耐心的回答我的问题，最后我想请问一下氯化钠在丙酮和乙酸乙酯中的溶解度，以便以后方便过滤氯化钠杂质

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28楼

引用MARK_GYC发表于27楼的内容

谢谢您一直耐心的回答我的问题，最后我想请问一下氯化钠在丙酮和乙酸乙酯中的溶解度，以便以后方便过滤氯化钠杂质

氯化钠很难溶于有机溶剂的

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29楼

可是楼主，氯化钠也溶于丙酮啊，（给您一张表格自己看一下）

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引用MARK_GYC发表于29楼的内容

可是楼主，氯化钠也溶于丙酮啊，（给您一张表格自己看一下）

氯化钠的话那就可以把高氯酸铵和氯化钠还有水的混合物冷冻，然后到零度的时候把水倒掉，然后加水重复一次（类似于氯酸钠制备氯酸钾）

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31楼

楼主真的挺耐心，一直为我解答关于AP各种问题，我为此表示诚挚的感谢！因为我本人去年刚刚入火箭燃料的坑（KNSU），后来听说AP基的推进剂性能更优越，于是打算想制备点APCP或者RAP燃料供发动机使用，但这个过程中我也产生了很多问题，幸好有楼主解答，要不然我就得多走弯路了……毕竟我才高二

附上几张我之前试车的照片

34184483367126136840441526199.mp4 点击下载 ‎

我想准备将AP系列燃料应用于PPR水管发动机（水泥喷管），不知道是否可行？谢谢！

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32楼

引用MARK_GYC发表于31楼的内容

楼主真的挺耐心，一直为我解答关于AP各种问题，我为此表示诚挚的感谢！因为我本人去年刚刚入火箭燃料的坑（KNSU），后来听说AP基的推进剂性能更优越，于是打算想制备点APCP或者RAP燃料供发动机使用，...

期待ap基燃料试车的照片，另外建议做个正经试车台，实在不行就挖个坑埋上，因为如果发动机失控乱窜就不好了。ap基的燃料要抽真空，如果有气泡很容易导致爆炸。

D864012

33楼

好的，因为我确实是“白手起家”地制作发动机，条件不太好，所以我干脆只能先用热熔胶把发动机黏在电子秤上试车，并且电子秤采样不精准，采样间隔大，造成了一些误差。今后我准备使用更高精度的推力采集设备，并且开始使用AP燃料（可能我会先试用NC纸张推进剂测试，魔术火纸）

我先从网上购买COD去除剂（氯酸钠，目前还未严格限制）并使用电解法将其变为高氯酸钠，最后再使用楼主您推荐的方法制备AP，至于副产物嘛……

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34楼

引用MARK_GYC发表于33楼的内容

好的，因为我确实是“白手起家”地制作发动机，条件不太好，所以我干脆只能先用热熔胶把发动机黏在电子秤上试车，并且电子秤采样不精准，采样间隔大，造成了一些误差。今后我准备使用更高精度的推力采集设备，并且开...

副产物也就是氯化钠什么的，能分离又没啥用

D864805

35楼

我有一个搬运过来与高氯酸铵性质相关的视频（原视频看我简介里的置顶评论链接）高氯酸铵的性质实验_哔哩哔哩_bilibili

希望可以对你起到帮助

1年4个月前 IP:河北

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36楼

引用MARK_GYC发表于35楼的内容

我有一个搬运过来与高氯酸铵性质相关的视频（原视频看我简介里的置顶评论链接）高氯酸铵的性质实验_哔哩哔哩_bilibili希望可以对你起到帮助

1年4个月前 IP:北京

D865043

37楼

话说楼主的实验进展的怎么样了，制备出来高纯度的高氯酸铵了吗 sticker

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38楼

引用MARK_GYC发表于37楼的内容

话说楼主的实验进展的怎么样了，制备出来高纯度的高氯酸铵了吗

以前做过了一次了

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